Preparation and Characterization of Bis[dihalo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes

Delrdre I. Arnold; F. Albert Cotton; Fritz E. Kühn

doi:10.1021/ic960325+

Preparation and Characterization of Bis[dihalo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes

Delrdre I. Arnold, F. Albert Cotton, Fritz E. Kühn

Texas A and M University

Research output: Contribution to journal › Article › peer-review

12 Scopus citations

Abstract

Complexes having the formula Mo₂X₄-dppa)₂ (X = Cl (2) Br (3); dppa = bis(diphenylphosphino)amine) can be synthesized by the reaction of Mo₂(OAc)₄ (OAc = μ-CH₃COO) with dppa and an excess of (CH₃ )₃SiX under reflux conditions. Both compounds were characterized by IR and UV/vis spectroscopy and by ³¹P{¹H} and ¹H NMR spectroscopy. Single-crystal diffraction studies afford the following pertinent crystal data for 2 and 3, respectively: monoclinic P2₁/c, a = 15.522(4) Å, b = 17.881(5) Å, c = 16.898(3) Å, β= 91.15(2)°, Z = 4; orthorhombic P2₁2₁2₁, a = 19.654(2), b = 19.865(2) c = 14.792(1), Z = 4. Both compounds exhibit significant torsion angles but, nevertheless, have comparatively short Mo-Mo bond distances (2, d(Mo-Mo) = 2.134(1) Å; 3, d(Mo-Mo) = 2.137(2) Å).

Original language	English
Pages (from-to)	5764-5769
Number of pages	6
Journal	Inorganic Chemistry
Volume	35
Issue number	20
DOIs	https://doi.org/10.1021/ic960325+
State	Published - 1996
Externally published	Yes

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@article{77170d20d2cc42a38c0a4960e7233d23,

title = "Preparation and Characterization of Bis[dihalo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes",

abstract = "Complexes having the formula Mo2X4-dppa)2 (X = Cl (2) Br (3); dppa = bis(diphenylphosphino)amine) can be synthesized by the reaction of Mo2(OAc)4 (OAc = μ-CH3COO) with dppa and an excess of (CH3 )3SiX under reflux conditions. Both compounds were characterized by IR and UV/vis spectroscopy and by 31P{1H} and 1H NMR spectroscopy. Single-crystal diffraction studies afford the following pertinent crystal data for 2 and 3, respectively: monoclinic P21/c, a = 15.522(4) {\AA}, b = 17.881(5) {\AA}, c = 16.898(3) {\AA}, β= 91.15(2)°, Z = 4; orthorhombic P212121, a = 19.654(2), b = 19.865(2) c = 14.792(1), Z = 4. Both compounds exhibit significant torsion angles but, nevertheless, have comparatively short Mo-Mo bond distances (2, d(Mo-Mo) = 2.134(1) {\AA}; 3, d(Mo-Mo) = 2.137(2) {\AA}).",

author = "Arnold, {Delrdre I.} and Cotton, {F. Albert} and K{\"u}hn, {Fritz E.}",

year = "1996",

doi = "10.1021/ic960325+",

language = "English",

volume = "35",

pages = "5764--5769",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "20",

}

TY - JOUR

T1 - Preparation and Characterization of Bis[dihalo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes

AU - Arnold, Delrdre I.

AU - Cotton, F. Albert

AU - Kühn, Fritz E.

PY - 1996

Y1 - 1996

N2 - Complexes having the formula Mo2X4-dppa)2 (X = Cl (2) Br (3); dppa = bis(diphenylphosphino)amine) can be synthesized by the reaction of Mo2(OAc)4 (OAc = μ-CH3COO) with dppa and an excess of (CH3 )3SiX under reflux conditions. Both compounds were characterized by IR and UV/vis spectroscopy and by 31P{1H} and 1H NMR spectroscopy. Single-crystal diffraction studies afford the following pertinent crystal data for 2 and 3, respectively: monoclinic P21/c, a = 15.522(4) Å, b = 17.881(5) Å, c = 16.898(3) Å, β= 91.15(2)°, Z = 4; orthorhombic P212121, a = 19.654(2), b = 19.865(2) c = 14.792(1), Z = 4. Both compounds exhibit significant torsion angles but, nevertheless, have comparatively short Mo-Mo bond distances (2, d(Mo-Mo) = 2.134(1) Å; 3, d(Mo-Mo) = 2.137(2) Å).

AB - Complexes having the formula Mo2X4-dppa)2 (X = Cl (2) Br (3); dppa = bis(diphenylphosphino)amine) can be synthesized by the reaction of Mo2(OAc)4 (OAc = μ-CH3COO) with dppa and an excess of (CH3 )3SiX under reflux conditions. Both compounds were characterized by IR and UV/vis spectroscopy and by 31P{1H} and 1H NMR spectroscopy. Single-crystal diffraction studies afford the following pertinent crystal data for 2 and 3, respectively: monoclinic P21/c, a = 15.522(4) Å, b = 17.881(5) Å, c = 16.898(3) Å, β= 91.15(2)°, Z = 4; orthorhombic P212121, a = 19.654(2), b = 19.865(2) c = 14.792(1), Z = 4. Both compounds exhibit significant torsion angles but, nevertheless, have comparatively short Mo-Mo bond distances (2, d(Mo-Mo) = 2.134(1) Å; 3, d(Mo-Mo) = 2.137(2) Å).

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U2 - 10.1021/ic960325+

DO - 10.1021/ic960325+

M3 - Article

AN - SCOPUS:0000549640

SN - 0020-1669

VL - 35

SP - 5764

EP - 5769

JO - Inorganic Chemistry

JF - Inorganic Chemistry

IS - 20

ER -

Preparation and Characterization of Bis[dihalo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes

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